CN101851099A - Preparation method for solid-phase sintered silicon carbide ceramics - Google Patents
Preparation method for solid-phase sintered silicon carbide ceramics Download PDFInfo
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- CN101851099A CN101851099A CN200910048846A CN200910048846A CN101851099A CN 101851099 A CN101851099 A CN 101851099A CN 200910048846 A CN200910048846 A CN 200910048846A CN 200910048846 A CN200910048846 A CN 200910048846A CN 101851099 A CN101851099 A CN 101851099A
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Abstract
The invention relates to a preparation method for solid-phase sintered silicon carbide ceramics, belonging to the field of silicon carbide ceramics. The invention uses SiC powder, B4C and graphite as sintering assistants and uses polyethylene glycol. The raw material powder is proportioned to slurry with weight percent of 35-60, SiC balls are used as grinding balls and are mixed with the slurry, the obtained slurry is dried and the obtained product is crushed and screened; the obtained powder is formed in a dry pressing way; and the formed product is sintered in Ar gas atmosphere. The density of the prepared solid-phase sintered silicon carbide ceramics is 2.75-3.10g/cm<3> and the bending strength is 250-500Mpa.
Description
Technical field
The present invention relates to preparation method, belong to the silicon carbide ceramics field with a kind of solid-phase sintered silicon carbide ceramics.
Background technology
Silicon carbide ceramics is with its excellent high-temperature stability, wear resistance, high thermal conductivity and be widely used in the industrial production.Wherein the silicon carbide ceramics of solid state sintering is because sintering aid content is very low, and the crystal boundary place can residual more low-melting material, and its physical and chemical performance has high-temperature stability, so the silicon carbide ceramics of solid state sintering has special using value.In most studies, solid-phase sintered silicon carbide ceramics with resol as binding agent, resol is as the part source of sintering aid carbon simultaneously, seldom use other binding agent, but resol is generally not molten by the aqueous solution, and therefore preparing in various moulding has its disadvantageous one side in the thyrite method.The present invention is a binding agent with polyoxyethylene glycol (PEG), has prepared the silicon carbide ceramics of different densities and mechanical property.
Summary of the invention
Preparation method of the present invention comprises the steps as follows:
(1) raw material of the present invention is the SiC powder, B
4C powder (accounting for the 0.05-5wt% of SiC powder quality) and graphite powder (accounting for the 0.5-10wt% of SiC powder quality) are sintering aid, polyoxyethylene glycol (PEG) is as the tackiness agent (accounting for the 0.01-20wt% of SiC powder quality) in the forming process of ceramics, and its molecular weight is 2000-8000.
Above-mentioned polyoxyethylene glycol preferably water dissolubility water polyoxyethylene glycol.
The preferred median size of above-mentioned SiC powder is 0.05-2 μ m's
(2) with water be solvent, material powder is made into the slurry of 35-60wt%, as mill ball, mix whole raw materials, all raw materials with the SiC ball: SiC ball=1: 0.5～5; Then with the oven dry of gained slurry, grinding and sieving.Behind the powder that obtains mixing, carry out dry-pressing formed with 20-100Mpa pressure; Sintering under normal pressure Ar gas atmosphere at last, sintering temperature is 1900-2300 ℃, soaking time is 30-240min.
By different content PEG and different soaking times, obtained the silicon carbide ceramics of different densities and mechanical property.Fig. 1-Fig. 2 is respectively the XRD curve of silicon carbide powder and carborundum sintered body, is mainly the 6H crystal formation of α-SiC from scheming silicon carbide powder as can be seen, behind 2100 ℃ high temperature sintering, has part 6H to be converted into the 4H crystal formation, and 4H is the high-temperature stable phase mutually.
Fig. 3-Fig. 4 shows the increase along with PEG content, and the density of carbofrax material and bending strength show and increase earlier the trend that afterwards reduces.
Fig. 5-Fig. 8 is a silicon carbide ceramics process corroded surface optical photograph under the different PEG content, therefrom have a large amount of bar-like grains to generate in the sintering process of silicon carbide ceramics as can be seen, but the generation of the fracture toughness property of the silicon carbide ceramics of different content explanation bar-like grains is not significantly increased the toughness of silicon carbide ceramics.
Mechanical property in sintering process under 1950 ℃ of carbofrax material normal temperature of obtaining of insulation 1h, increase along with PEG content, the density of carbofrax material and mechanical property change little, but compare with carbofrax material with the PEG content of content, along with holding time prolonging, the silicon carbide whisker particle size increases, reached 0.1-0.2mm (Fig. 9-Figure 11), this explanation at a lower temperature, the rate of diffusion of silicon carbide ceramics crystal boundary is still bigger, the mechanical property of material compare with the mechanical property of 1950 ℃ of carbofrax materials of obtaining of insulation 15min in sintering process reduce bigger.
In sum, the present invention is that binding agent is to prepare mechanical property solid-phase sintered silicon carbide ceramics preferably with water-soluble PEG, and it is for being that the forming method of dispersion medium provides experiment basis with water.
Description of drawings
Fig. 1 is the XRD curve of silicon carbide powder.
Fig. 2 is the XRD curve of carborundum sintered body.
Fig. 3 is a silicon carbide ceramics density under the different PEG content.
Fig. 4 is a silicon carbide ceramics flexural strength under the different PEG content.
Fig. 5-Fig. 8 is a silicon carbide ceramics surface optical photo under the different PEG content, and PEG content is respectively 0,3%, 5%, 10%.(1950℃-15min)
Fig. 9-Figure 11 is a silicon carbide ceramics surface optical photo under the different PEG content, and PEG content is respectively 3%, 5%, 10%.(1950℃-60min)
Embodiment
Further specify characteristics of the present invention below by specific embodiment, but the present invention is confined to embodiment by no means.
Embodiment 1
SiC, sintering aid B
4C (0.2wt%) is total to 100g with graphite (4wt%), and PEG is 3g (3wt% of powder), and water is solvent, after PEG is dissolved in deionized water, powder being made into the slurry that solid content is 45wt%, is ball-milling medium with SiC ball 200g, mix 24h, then in thermostat container till 80 ℃ of oven dry.Grind then, through after the 100 purpose sieve, the powder that obtains is the 60Mpa pressure forming on vulcanizing press again.
Sintering under normal pressure Ar gas atmosphere, sintering temperature is 2100 ℃, and soaking time is 1h, wherein is incubated 15min in the time of 1950 ℃, and the silicon carbide ceramics density that obtains is 3.04gcm
-3, bending strength is 453.9Mpa.
Embodiment 2
SiC, sintering aid B4C (0.2wt%) are total to 100g with graphite (4wt%), and PEG is 5g (5wt% of powder), and water is solvent, PEG and powder are made into the slurry that solid content is 50wt%, with SiC ball 200g is ball-milling medium, mixes 24h, then in thermostat container till 80 ℃ of oven dry.Grind then, through after the 100 purpose sieve, the powder that obtains is the 60Mpa pressure forming on vulcanizing press again.
Sintering under normal pressure Ar gas atmosphere, sintering temperature is 2100 ℃, and soaking time is 1h, wherein is incubated 60min in the time of 1950 ℃, and the silicon carbide ceramics density that obtains is 2.78gcm
-3, bending strength is 273.7Mpa.
Claims (7)
1. the preparation method of a solid-phase sintered silicon carbide ceramics is characterized in that, comprises the steps:
(1) selects the SiC powder for use, account for the B of SiC powder quality 0.05-5wt%
4C, the graphite that accounts for SiC powder quality 0.5-10wt% is sintering aid, accounts for the polyoxyethylene glycol of SiC powder quality 0.01-20wt%;
(2) material powder is made into the slurry of 35-60wt%, mixes as mill ball, all raw materials with the SiC ball: SiC ball=1: 0.5～5, then with the oven dry of gained slurry, grinding and sieving;
(3) powder that obtains is dry-pressing formed with 20-100Mpa; Sintering under Ar gas atmosphere.
2. by the preparation method of the described a kind of solid-phase sintered silicon carbide ceramics of claim 1, it is characterized in that the molecular weight of polyoxyethylene glycol is 2000-8000.
3. by the preparation method of claim 1 or 2 described a kind of solid-phase sintered silicon carbide ceramics, it is characterized in that selected solvent is ethanol or water.
4. by the preparation method of claim 3 or described a kind of solid-phase sintered silicon carbide ceramics, it is characterized in that selected solvent is a water.
5. by the preparation method of claim 1 or 2 described a kind of solid-phase sintered silicon carbide ceramics, it is characterized in that, polyoxyethylene glycol be water-soluble water polyoxyethylene glycol.
6. by the preparation method of the described a kind of solid-phase sintered silicon carbide ceramics of claim 2, it is characterized in that the median size of SiC powder is 0.05-2 μ m.
7. by the preparation method of the described a kind of solid-phase sintered silicon carbide ceramics of claim 2, it is characterized in that sintering temperature is 1900-2300 ℃, soaking time is 30-240min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478104A (en) * | 2015-08-24 | 2017-03-08 | 中国科学院上海硅酸盐研究所 | A kind of method that new type gel cast prepares silicon carbide ceramics with reference to solid-phase sintering |
| CN108558406A (en) * | 2018-05-03 | 2018-09-21 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of silicon carbide ceramics grinding bead |
| CN108585875A (en) * | 2018-04-03 | 2018-09-28 | 中国科学院上海硅酸盐研究所 | A kind of large scale, high strength graphite alkene nanometer sheet/composite material of silicon carbide and preparation method thereof |
| CN108752002A (en) * | 2018-07-27 | 2018-11-06 | 中国人民解放军国防科技大学 | SiC ceramic-based hot bending die and preparation method thereof |
| CN113416076A (en) * | 2021-08-16 | 2021-09-21 | 东北大学 | Preparation method of self-reinforced silicon carbide ceramic material |
-
2009
- 2009-04-03 CN CN200910048846A patent/CN101851099A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478104A (en) * | 2015-08-24 | 2017-03-08 | 中国科学院上海硅酸盐研究所 | A kind of method that new type gel cast prepares silicon carbide ceramics with reference to solid-phase sintering |
| CN106478104B (en) * | 2015-08-24 | 2019-04-16 | 中国科学院上海硅酸盐研究所 | A kind of method that new type gel casting combines solid-phase sintering to prepare silicon carbide ceramics |
| CN108585875A (en) * | 2018-04-03 | 2018-09-28 | 中国科学院上海硅酸盐研究所 | A kind of large scale, high strength graphite alkene nanometer sheet/composite material of silicon carbide and preparation method thereof |
| CN108585875B (en) * | 2018-04-03 | 2021-01-12 | 中国科学院上海硅酸盐研究所 | Large-size and high-strength graphene nanosheet/silicon carbide composite material and preparation method thereof |
| CN108558406A (en) * | 2018-05-03 | 2018-09-21 | 苏州卫优知识产权运营有限公司 | A kind of preparation process of silicon carbide ceramics grinding bead |
| CN108752002A (en) * | 2018-07-27 | 2018-11-06 | 中国人民解放军国防科技大学 | SiC ceramic-based hot bending die and preparation method thereof |
| CN108752002B (en) * | 2018-07-27 | 2020-08-07 | 中国人民解放军国防科技大学 | SiC ceramic-based hot bending die and preparation method thereof |
| CN113416076A (en) * | 2021-08-16 | 2021-09-21 | 东北大学 | Preparation method of self-reinforced silicon carbide ceramic material |
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Application publication date: 20101006 |